Process For Making Form I Of Olanzapine
a technology of dihydrate c and olanzapine, which is applied in the field of new dihydrate c of olanzapine, can solve the problems of difficult removal of impurity c and increase of impurity level
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example 1
Preparation of Crude Olanzapine Form I
[0033] Crude Olanzapine (30.0 g) is added into dichloromethane (180 ml). The reaction mixture is refluxed at 35-40° C. for a period of 15-20 min. When complete dissolution occurs, activated carbon (1.20 g) is added and the reaction mixture is then refluxed at 35-40° C. for 15 min. The solution is then filtered through hy-flo bed and the bed is washed with dichloromethane (30 ml). The filtrate is then slowly cooled to 0-5° C. and then maintained at 0-5° C. for 5 h to complete the crystallization. The content is then filtered, washed with chilled (0-5°) dichloromethane (30 ml) and dried at 70° C.-75° C. under vacuum for 12 hours (Yield 14 g) to give Olanzapine Form I. Dichloromethane content 620 ppm. Impurity C is 0.2% w / w.
example 2
Preparation of Olanzapine Dihydrate C
[0034] Olanzapine Form—I (10 g) is suspended in water (30 ml) and stirred at 30 to 35° C. over a period of 30 minutes. The slurry is then filtered and washed with water (50 ml) and suck dried. The product obtained is dried at 30 to 35° C. for 24 hrs (Yield: 9.5 g). The moisture content of the product is 10.2%.
[0035] The product is examined by powder x-ray crystallography, infrared spectroscopy and differential scanning calorimetry to identify the crystal form (FIGS. 1 to 3). The product is examined by powder x-ray crystallography, infrared spectroscopy and differential scanning calorimetry to identify the crystal form (FIGS. 1 to 3).
example 3
Preparation of Form I of Olanzapine
[0036] The Olanzapine Dihydrate C (10 g) is dried at 60° C. to 70° C. under vacuum for 3 to 4 hours (Yield: 8.5 g) to obtain substantially pure Olanzapine Form I. The moisture content of the product is 0.2% and dichloromethane is 112 ppm. Impurity C content is 0.08% w / w. Thus it is clear that producing Olanzapine Form I by following the process as invented by the present applicant [eg. 3] results in lesser DCM content as well as lower impurity C levels.
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